# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'T M Klapotke' _publ_contact_author_email TMK@CUP.UNI-MUENCHEN.DE _publ_section_title ; First structural characterization of solvate-free silver dinitramide, Ag[N(NO2)2] ; loop_ _publ_author_name 'T M Klapotke' 'Burkhard Krumm' 'Matthias Scherr' # Attachment 'tmk_AgDN.cif' data_dx152 _database_code_depnum_ccdc_archive 'CCDC 693547' _audit_update_record ; 'Thu Apr 17 15:51:14 2008' ; _chemical_name_common 'silver dinitramide' _chemical_compound_source ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_special_details ? #:---------------------------------------------------------------------------- #:---------------------------DATA COLLECTION---------------------------------- #:---------------------------------------------------------------------------- _audit_author_name 'Scherr, Matthias' _audit_creation_date ; 'Thu Apr 17 14:30:09 2008' ; _diffrn_ambient_temperature 200(2) #?# in K _diffrn_source_type 'Spellman generator' _diffrn_source_power 2.00_kW _diffrn_source_voltage 50_kV _diffrn_source_current 40_mA _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_collimation '0.5 mm collimator' _diffrn_measurement_device_type 'Oxford Xcalibur3 CCD area-detector' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 15.9809 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 0.00 51.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.7619 45.0000 240.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 2 omega -44.00 6.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.7619 -45.0000 240.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 3 omega -93.00 -43.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.7619 -45.0000 240.0000 0.0000 0.0000 50 #__ type_ start__ end____ width___ exp.time_ 4 omega -34.00 -6.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -20.7619 131.0000 -20.0000 0.0000 0.0000 28 #__ type_ start__ end____ width___ exp.time_ 5 omega -46.00 -5.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 20.9181 138.0000 -93.0000 0.0000 0.0000 41 #__ type_ start__ end____ width___ exp.time_ 6 omega 39.00 67.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 20.9181 75.0000 240.0000 0.0000 0.0000 28 ; _kl_diffrn_measurement_detector_distance 50 _diffrn_special_details ? _diffrn_orient_matrix_type ? _diffrn_orient_matrix_UB_11 0.0340793073 _diffrn_orient_matrix_UB_12 -0.0407107920 _diffrn_orient_matrix_UB_13 0.0397789750 _diffrn_orient_matrix_UB_21 0.0188545197 _diffrn_orient_matrix_UB_22 0.0602411144 _diffrn_orient_matrix_UB_23 0.0274639750 _diffrn_orient_matrix_UB_31 -0.1158551433 _diffrn_orient_matrix_UB_32 -0.0021844234 _diffrn_orient_matrix_UB_33 0.0161805900 loop_ _reflns_scale_group_code _reflns_scale_meas_F ? ? _cell_length_a 5.8040(4) _cell_length_b 9.7496(6) _cell_length_c 13.9105(8) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 787.15(9) _cell_measurement_temperature 200(2) #?# in K _cell_measurement_reflns_used 1590 _cell_measurement_theta_min 3.7954 _cell_measurement_theta_max 28.7395 _cell_special_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist ? ? ? ? #:---------------------------------------------------------------------------- #:---------------------------ABSORPTION CORRECTION---------------------------- #:---------------------------------------------------------------------------- _exptl_absorpt_coefficient_mu 5.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2215 _exptl_absorpt_correction_T_max 0.6700 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; #:---------------------------------------------------------------------------- #:------------------------REFLECTION DATA ANALYSIS---------------------------- #:---------------------------------------------------------------------------- _diffrn_reflns_number 2878 #xl _diffrn_reflns_av_R_equivalents 0.0267 #xl _diffrn_reflns_av_sigmaI/netI 0.0283 #xl _diffrn_reflns_limit_h_min -6 #xl _diffrn_reflns_limit_h_max 7 #xl _diffrn_reflns_limit_k_min -9 #xl _diffrn_reflns_limit_k_max 12 #xl _diffrn_reflns_limit_l_min -17 #xl _diffrn_reflns_limit_l_max 17 #xl _diffrn_reflns_theta_min 4.18 #xl _diffrn_reflns_theta_max 25.99 #xl _diffrn_measured_fraction_theta_max 0.994 #xl _diffrn_reflns_theta_full 25.99 #xl _diffrn_measured_fraction_theta_full 0.994 #xl #:---------------------------------------------------------------------------- #:---------------------STRUCTURE SOLUTION AND REFINEMENT---------------------- #:---------------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _reflns_number_total 765 #xl _reflns_number_gt 581 #xl _reflns_threshold_expression >2sigma(I) #xl _reflns_special_details ? _refine_ls_structure_factor_coef Fsqd #xl _refine_ls_matrix_type full #xl _refine_ls_weighting_scheme calc #xl _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' #xl _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none #xl _refine_ls_extinction_coef ? #xl _refine_ls_abs_structure_details ? #xl _refine_ls_abs_structure_Flack ? #xl _refine_ls_number_reflns 765 #xl _refine_ls_number_parameters 73 #xl _refine_ls_number_restraints 0 #xl _refine_ls_R_factor_all 0.0469 #xl _refine_ls_R_factor_gt 0.0352 #xl _refine_ls_wR_factor_ref 0.0965 #xl _refine_ls_wR_factor_gt 0.0906 #xl _refine_ls_goodness_of_fit_ref 1.108 #xl _refine_ls_restrained_S_all 1.108 #xl _refine_ls_shift/su_max 0.000 #xl _refine_ls_shift/su_mean 0.000 #xl _refine_diff_density_max 1.418 #xl _refine_diff_density_min -1.696 #xl _refine_diff_density_rms 0.186 #xl _refine_special_details ? #:---------------------------------------------------------------------------- #:-----------------------------REFERENCES------------------------------------- #:---------------------------------------------------------------------------- _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (G. M. Sheldrick. University of G\"ottingen, Germany, 1997)' _computing_structure_refinement 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1996)' _computing_publication_material 'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)' #:---------------------------------------------------------------------------- #:---------------------TABLES AND GEOMETRICAL DATA---------------------------- #:---------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.0932(7) -0.1860(5) 0.3704(3) 0.0179(10) Uani 1 1 d . . . N2 N 0.1560(7) -0.1429(4) 0.4613(3) 0.0167(9) Uani 1 1 d . . . N3 N 0.0984(7) -0.0879(5) 0.3005(4) 0.0190(10) Uani 1 1 d . . . O1 O 0.1102(7) -0.2277(4) 0.5243(3) 0.0239(9) Uani 1 1 d . . . O2 O 0.2608(6) -0.0362(4) 0.4779(3) 0.0226(8) Uani 1 1 d . . . O3 O 0.0885(7) -0.1341(5) 0.2187(3) 0.0281(10) Uani 1 1 d . . . O4 O 0.0969(7) 0.0368(4) 0.3166(3) 0.0300(10) Uani 1 1 d . . . Ag1 Ag 0.08057(9) 0.10455(5) 0.14168(3) 0.0348(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.026(2) 0.012(2) 0.016(2) 0.003(2) -0.0030(19) -0.0022(18) N2 0.014(2) 0.020(2) 0.016(2) 0.001(2) -0.0011(19) 0.0018(19) N3 0.013(2) 0.024(3) 0.020(3) 0.0046(19) -0.0005(19) 0.0002(18) O1 0.026(2) 0.026(2) 0.020(2) 0.0086(18) 0.0000(17) -0.0001(17) O2 0.024(2) 0.0193(19) 0.0240(19) -0.0028(17) -0.0058(18) -0.0046(17) O3 0.025(2) 0.044(3) 0.0155(19) -0.001(2) -0.0021(17) 0.0028(19) O4 0.044(2) 0.018(2) 0.028(2) 0.0082(19) -0.001(2) 0.0001(19) Ag1 0.0488(4) 0.0297(4) 0.0259(3) 0.0129(2) 0.0128(2) 0.0151(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 N3 1.364(6) . ? N1 N2 1.382(6) . ? N1 Ag1 2.284(4) 4_545 ? N2 O2 1.227(6) . ? N2 O1 1.233(5) . ? N3 O3 1.226(6) . ? N3 O4 1.236(6) . ? O2 Ag1 2.546(3) 2 ? O3 Ag1 2.562(4) . ? O4 Ag1 2.524(4) . ? Ag1 N1 2.284(4) 4 ? Ag1 O2 2.546(3) 2_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 N1 N2 115.7(4) . . ? N3 N1 Ag1 125.7(3) . 4_545 ? N2 N1 Ag1 117.1(3) . 4_545 ? O2 N2 O1 122.8(4) . . ? O2 N2 N1 124.1(4) . . ? O1 N2 N1 112.9(4) . . ? O3 N3 O4 122.0(5) . . ? O3 N3 N1 113.8(4) . . ? O4 N3 N1 124.1(5) . . ? N2 O2 Ag1 97.2(3) . 2 ? N3 O3 Ag1 93.2(3) . . ? N3 O4 Ag1 94.8(3) . . ? N1 Ag1 O4 108.77(14) 4 . ? N1 Ag1 O2 109.14(14) 4 2_554 ? O4 Ag1 O2 141.34(13) . 2_554 ? N1 Ag1 O3 148.31(14) 4 . ? O4 Ag1 O3 50.09(14) . . ? O2 Ag1 O3 97.45(12) 2_554 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 N1 N2 O2 -16.8(7) . . . . ? Ag1 N1 N2 O2 176.2(4) 4_545 . . . ? N3 N1 N2 O1 168.1(4) . . . . ? Ag1 N1 N2 O1 1.0(5) 4_545 . . . ? N2 N1 N3 O3 165.8(4) . . . . ? Ag1 N1 N3 O3 -28.4(5) 4_545 . . . ? N2 N1 N3 O4 -19.0(7) . . . . ? Ag1 N1 N3 O4 146.8(4) 4_545 . . . ? O1 N2 O2 Ag1 16.1(5) . . . 2 ? N1 N2 O2 Ag1 -158.5(4) . . . 2 ? O4 N3 O3 Ag1 1.3(5) . . . . ? N1 N3 O3 Ag1 176.6(3) . . . . ? O3 N3 O4 Ag1 -1.3(5) . . . . ? N1 N3 O4 Ag1 -176.1(4) . . . . ? N3 O4 Ag1 N1 153.2(3) . . . 4 ? N3 O4 Ag1 O2 -38.5(4) . . . 2_554 ? N3 O4 Ag1 O3 0.7(2) . . . . ? N3 O3 Ag1 N1 -56.9(4) . . . 4 ? N3 O3 Ag1 O4 -0.7(2) . . . . ? N3 O3 Ag1 O2 155.8(3) . . . 2_554 ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? _geom_special_details ? #:---------------------------------------------------------------------------- #:--------------------------ARCHIVING AND CHECKING---------------------------- #:---------------------------------------------------------------------------- _audit_block_code AgDN_dx152_Scherr _audit_creation_method 'form98_non/compatible with shelxl97-2' _chemical_name_systematic ? _chemical_formula_moiety 'Ag N3 O4' _chemical_formula_sum 'Ag N3 O4' _chemical_formula_weight 213.886 _chemical_melting_point ? _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 3.6097(6) _exptl_crystal_F_000 800